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EXPERIMENTAL
Experimental
Chapter 3: Experimental
3.0 Experimental
In the present work effect of type of polyol, diisocyanate, diacrylate and acrylate on
properties of EB curable urethane acrylate coatings were studied. The EB coating
system properties were also studied using nanoalumina and nanosilica.
3.1 Materials
The polyols used for present study are pentaerythritol, glycerol, 1,4-butanediol, 1,6hexanediol, NPG were supplied by s.d.fine-chem limited, Mumbai and of laboratory
reagent (LR) grade. Pentaerythritol, procured from Asian PPG, Mumbai. Adipic acid
supplied by s.d.fine-chem was also of LR grade. IPDI, TDI and MDI were supplied
by Merck, India and were of LR grade. HEA, TMPTA and EGDMA were supplied by
ChemFine Int.Co.,Ltd (China).
Nanosilica and nanoalumina dispersion were provided by BYK, Mumbai. Catalyst
Dibutyl tindilaurate (DBTDL) was obtained by Maharashtra organic chemicals.
Xylene, toluene and DMSO were of LR grade from s.d.fine-chem Ltd, Mumbai.
3.2 Experimental
3.2.1 Raw material analysis
The raw materials used for present work were assessed for their purity (%). The
polyols were analyzed on the basis of hydroxyl value, diisocyanates were analyzed by
determination of NCO (%) and adipic acid was analyzed by determination of acid
value.
3.2.2 Determination of percentage purity of Pentaerythritol
Weigh 2 gm of the sample into a 100 ml flask. Dissolve in minimum quantity of water
and diluted to 100 ml. Mix 10 ml of this solution with 1 ml of p-nitrobenzaldehyde
distilled (prepared by dissolving 1gm p-nitrobenzaldehyde in 5 ml of methanol and 2
ml of concentrated HCl) heat to boil under reflux condition in water bath for 1hr 30
min in a 250 ml flask. Cool and neutralize the contents with NaOH solution. Add
sufficient quantity of methanol. Boil the contents for a short time. Cool and filter
under vacuum. Wash the residue and weigh.
69
Experimental
Purity of monopenta =
100 = 98.55 %
.
.
= 98.43 %
70
Experimental
= 950.847 %
Experimental
Average OH-value =
= 938.29
Purity of 16-hexanediol =
Purity = 938.29/ 950.847 = 0.9868 x 100 = 98.68 %
Actual OH-value =
1225.51
Actual OH-value =
= 1016.34
72
Experimental
Acid value =
.
.
768.49 %
762.70
99.20 %
Purity =
483.62
.
.
.
.
= 478.09
98.86 %
73
Experimental
431.54
.
.
.
.
422.43
Purity =
97.89 %
74
Experimental
40.73 %
103.12
103.12
Purity =
82.50 %
Actual value
Weight of TDI = 1.26 g
Blank = 41.2
Burette reading = 30.2 ml
NCO content =
50.08 %
83.86
100
.
.
75
96.39%
Experimental
43.31 %
100
96.98
.
.
.
76
87.76 %
Experimental
+ 4 H2O
Polyester polyol
77
Experimental
78
Experimental
PENTA
Adipic
1,6-
acid
Hexanediol
Pgel
(%)
(C)
(%)
moles
moles
moles
PP1
0.5
68
1.0
146
0.5
59
xylene
0.1
140
100
PP2
0.5
68
1.0
146
0.5
59
DMSO
0.1
153
100
PP3
0.5
68
1.0
146
0.5
59
DMF
0.1
189
100
PP4
0.5
68
1.0
146
0.5
59
0.1
189
100
PP5
0.5
68
1.0
146
0.5
59
0.05
190
100
PP6
0.5
68
1.0
146
0.5
59
0.05
160
100
PENTA
Adipic
1,6-
acid :
diol :
Pgel
acid
Hexanediol
polyol
tetrol
(%)
1.0:2.0
87.34
moles
moles
moles
PP7
0.50
68
1.0
146
0.25
PP8
0.40
54.4
1.0
146
0.50
59
1.0:0.9
1.25:1.0
PP9
0.20
27.2
1.0
146
1.0
118
1.0:1.2
5.0:1.0
109
PP10
0.16
21.8
1.0
146
1.0
118
1.0:1.16 6.25:1.0
108
79
g
29.5 1.0:0.75
Experimental
3.3.2 Synthesis of Polyester polyol from Glycerol, adipic acid and 1, 6-hexanediol
The polyester polyols were synthesized with adipic acid, 1, 6-hexanediol and glycerol.
The schematic representation of polyester polyol formation are depicted in Figure 3.2
+ 3H2O
Polyester polyol
The above polyol is represented as
HO
OH
OH
The reactions were carried out in nitrogen atmosphere using xylene as azeotropic
solvent for removal of water from reaction mixture. The progress of reaction was
monitored by amount of water of reaction as well as acid value. The reactions were
terminated when required water of reaction is collected azetropically and acid value
reached to 10 mg of KOH/gm of resin. The mole ratio was decided for the hydroxyl to
80
Experimental
Table 3.3: Typical formulation for polyester polyols with varying acid to
hydroxyl ratio as well as varying ratio of diol to triol
Batch
Glycerol
Adipic
1,6-
acid :
diol :
Pgel
acid
Hexanediol
polyol
triol
(%)
moles
moles
moles
GP1
0.2
18.6
1.0
146
0.9
94.4
1.0:1.1
4.5:1.0
105
GP2
0.3
27.9
1.0
146
0.9
94.4
1.0:1.2
3.0:1.0
110
GP3
0.4
37.2
1.0
146
0.9
94.4
1.0:1.3
2.25:1.0
115
3.3.3 Synthesis of Polyester polyol from 1, 4-butanediol, adipic acid and 1, 6hexanediol
The polyester polyols were synthesized with adipic acid, 1, 6-hexanediol and 1,4butanediol.
The schematic representation of polyester polyol formation are depicted in Figure 3.3
81
Experimental
Figure 3.3: Two-Dimensional theoretical representation of the synthesis of 1,4butanediol co-polyester polyol.
The reactions were carried out in nitrogen atmosphere using xylene as azeotropic
solvent for removal of water from reaction mixture. The progress of reaction was
monitored by amount of water of reaction as well as acid value. The reactions were
terminated when required water of reaction is collected azetropically and acid value
reached to 10 mg of KOH/gm of resin. The mole ratio was decided for the hydroxyl to
be approximately around 160-170 mg of KOH/gm of resin. The typical formulations
with varying concentration of 1, 6-hexanediol, glycerol and acid: hydroxyl ratios are
presented in Table 3.4.
82
Experimental
Table 3.4: Typical formulation for polyester polyols with varying acid to
hydroxyl ratio as well as varying type of diol
Batch
1,4-
Adipic
1,6-
acid :
Pgel
butanediol
acid
Hexanediol
polyol
(%)
moles
moles
moles
BP1
0.6
54
1.0
146
0.7
82.6
1.0:1.3
115
BP2
0.7
63
1.0
146
0.7
82.6
1.0:1.4
119
BP3
0.8
72
1.0
146
0.7
82.6
1.0:1.5
125
3.3.4 Synthesis of Polyester polyol from NPG, adipic acid and 1, 6-hexanediol
The polyester polyols were synthesized with adipic acid, 1, 6-hexanediol and NPG.
The schematic representation of polyester polyol formation are depicted in Figure 3.4
The reactions were carried out in nitrogen atmosphere using xylene as azeotropic
solvent for removal of water from reaction mixture. The progress of reaction was
monitored by amount of water of reaction as well as acid value. The reactions were
terminated when required water of reaction is collected azetropically and acid value
reached to 10 mg of KOH/gm of resin. The mole ratio was decided for the hydroxyl to
be approximately around 160-170 mg of KOH/gm of resin. The typical formulations
with varying concentration of 1, 6-hexanediol, NPG and acid: hydroxyl ratios are
presented in Table 3.5.
83
Experimental
Table 3.5: Typical formulation for polyester polyols with varying acid to
hydroxyl ratio as well as varying ratio of diol
Batch
Neopentyl
Adipic
1,6-
acid :
Pgel
glycol
acid
Hexanediol
polyol
(%)
moles
moles
moles
NP1
0.6
62.4
1.0
146
0.7
82.6
1.0:1.3
115
NP2
0.7
72.8
1.0
146
0.7
82.6
1.0:1.4
119
NP3
0.8
83.2
1.0
146
0.7
82.6
1.0:1.5
125
84
Experimental
85
Experimental
The typical formulations and mode of reaction of urethane acrylate are described as
follows.
3.4.1 Synthesis of urethane acrylate using PENTA polyol, diisocyanate and
hydroxyl acrylate
A three neck flask equipped with nitrogen inlet, condenser and addition funnel is
placed in a water bath. Diisocyanate is charged in the reactor, and dropwise addition
of hydroxyl acrylate.
determined. Further the dropwise addition of polyester polyol. The reaction is carried
out in an inert atmosphere. The reaction was performed till the resultant had an
isocyanate value 0.5%. The reaction mode is as shown in Figure 3.5 and Figure
3.6.
O
NCO
NCO
HO
CH2
O
HEA
IPDI
NCO
NH
CH2
Experimental
Isocyanate
Batch
PUA1
Hydroxyl
Solvent
Catalyst
Temp
acrylate
(wt %)
(wt %)
(C)
0.01
30
Xylene-
0.01
20
0.0097
30
Xylene-
0.0097
30
0.342
30
0.342
20
0.342
20
0.343
20
0.366
20
moles
moles
moles
0.015
5.19
MDI-0.03
3.09
HEMA-
1.99
0.015
PUA2
0.01
3.46
MDI-0.02
2.06
HEMA-
1.33
0.01
PUA3
0.015
5.19
TDI-0.03
2.52
HEMA-
1.37(20)
1.99
0.015
PUA4
0.015
5.19
TDI-0.03
2.52
HEMA-
1.99
0.015
PUA5
0.5
172.92
TDI-1.2
100.06
HEMA-
0.097(10)
69.06
0.6
PUA6
0.5
172.92
TDI-1.2
100.06
HEMA-
69.06
0.6
PUA7
0.6
207.50
TDI-1.2
100.06
HEA-0.6
Xylene68.40(20)
Xylene68.40(20)
70.40
Xylene75.59(20)
PUA8
0.5
172.92
TDI-1.2
100.06
HEA-0.6
70.40
Xylene68.68(20)
PUA9
0.6
207.50
TDI-1.2
100.06
HEA-0.5
58.67
Acetone36.62(10)
PUA10
0.6
207.50
IPDI-1.2
116.38
HEMA-
79.68
0.404
55
0.6
PUA11
0.6
207.50
IPDI-1.2
116.38
HEA-0.6
70.40
0.394
55
PUA12
0.7
207.50
IPDI-1.4
135.77
HEA-0.7
82.14
0.425
55
PUA13
0.9
311.25
IPDI-1.6
155.17
HEA-0.7
82.14
0.549
55
Not e: MDI (Methylene biphenyl diisocyanate), TDI(Toluene diisocyanate), IPDI (Isophorone diisocyanate), HEA
(hydroxy ethyl acrylate), HEMA (hydroxy ethyl methacrylate)
87
Experimental
determined. Further the dropwise addition of polyester polyol. The reaction is carried
out in an inert atmosphere. The reaction was performed till the resultant had an
isocyanate value 0.5%.
88
Experimental
Isocyanate
Batch
GUA1
Hydroxyl
Solvent
Catalyst
Temp
acrylate
(wt %)
(wt %)
(C)
Acetone-
0.032
20
0.032
20
moles
moles
moles
0.5
173.26
TDI-1.0
83.86
HEA-0.5
58.67
31.58
GUA2
0.5
173.26
TDI-1.0
83.86
HEMA-
66.4
0.5
GUA3
0.5
173.26
IPDI-1.0
96.98
HEMA-
Acetone32.35
66.4
0.034
55
58.67
0.033
55
0.5
GUA4
0.5
173.26
IPDI-1.0
96.98
HEA-0.5
89
Experimental
IPDI
moles
g
Polyol
moles
g
HEA
moles
g
Catalyst
(wt %)
BUA1
1.0
96.98
0.5
169.53
0.5
58.67
0.033
BUA2
2.0
193.96
1.0
339.05
1.0
117.34
0.065
polyester polyol
90
Experimental
IPDI
moles
g
Polyol
moles
g
HEA
moles
G
Catalyst
(wt %)
NUA1
1.0
96.98
0.5
170.71
0.5
58.67
0.33
NUA2
2.0
193.96
1.0
341.43
1.0
117.34
0.65
Experimental
and
viscosity.
Characterization
was
done
by
FTIR,
NMR,
UV
spectrophotometer, GPC.
3.5.1.1 Acid Value
It is defined as milligrams of KOH required to neutralize the free carboxylic acid
present in one gram of resin. Acid value of the obtained polyester polyol was
measured according to ASTM D 1639-70 during the reaction.
3.5.1.2 Hydroxyl Value
The hydroxyl value is defined as the number of milligrams of KOH required to
esterifies the hydroxyl (-OH) groups. The hydroxyl value of polyester polyols was
determined as per ISO 4629-1978(E).
3.5.1.3 Viscosity by Brookfield (ASTM D 1638 -74)
Viscosities were measured using a Brookfield viscometer. The viscosity in centipoise
was found by multiplying the reading by the factor (f) that goes with the spindle and
speed used.
Viscosity = Reading x f.
3.5.1.4 FTIR analysis
The FTIR spectra were recorded using a NaCl cell on a Perkin-Elmer spectrum BX
FT-IR (USA) spectrophotometer taking 256 scans. The transmission mode was used
and the wave number range was set from 400-4000 cm-1. Fourier transform infrared
(FTIR) method was employed to study the formation of polyester polyol, urethane
acrylate and the electron beam curing of the samples.
3.5.1.5 1H NMR and 13C NMR analysis
1
H NMR and 13C NMR was recorded on a Bruker Avnace (Germany) with 5 mm BBI
Experimental
Experimental
Experimental
Films for FTIR, gel fraction were cured on glass plates, were peeled off to conduct
these studies.
Table3.10 Typical UV curing formulations with photoinitiator, oligomer and
reactive diluent
Batch
Oligomer
Reactive diluent
Photoinitiator
(wt %)
(HEA) wt %
(wt %)
90
10
5%
PUA2
PUA6
PUA7
PUA8
PUA9
PUA10
PUA11
PUA12
No. of Passes
PUA2
PUA6
PUA7
PUA8
PUA9
PUA10
PUA11
PUA12
7
95
Experimental
Urethane acrylate
Adhesion
oligomer (%)
Promoter (wt %)
95
0.5
05
05
05
90
0.5
10
10
10
85
0.5
15
15
15
80
0.5
20
20
20
75
0.5
25
25
25
TMPTA
EGDMA
HEA
Table 3.13 Typical UV curing with varying irradiation time and reactive diluents
TMPTA
%
EGDMA
PI
No. of
Conveyor
(%)
Passes
speed
4.2
10
15
20
25
HEA
PI
No. of
Conveyor
(%)
Passes
speed
5.0
4.2
10
6.1
15
6.1
20
6.1
25
PI
No. of
Conveyor
(%)
Passes
speed
4.2
5.0
10
4.2
6.1
15
4.2
6.1
20
5.1
6.1
25
5.1
96
Experimental
Table 3.15. For UV curing only basic coating properties like flexibility and impact
was checked. The thickness of the cured coating was found to be approx. 100 m.
Table 3.14: Typical UV curing formulations with varying ratio of photoinitiator,
oligomer (GUA4) and reactive diluent
Urethane acrylate
TMPTA (%)
oligomer (%)
Adhesion
PI (wt %)
promoter
100
00
0.5
95
05
0.5
90
10
0.5
85
15
0.5
80
20
0.5
75
25
0.5
6.0
6.0
10
6.0
15
5.0
20
5.0
25
5.0
97
Experimental
TMPTA (%)
oligomer (%)
Adhesion
PI
promoter (wt %)
(wt %)
100
00
0.5
90
10
0.5
80
20
0.5
75
25
0.5
5.0
10
5.0
20
5.0
25
5.0
98
Experimental
TMPTA (%)
oligomer (%)
Adhesion
PI (wt %)
promoter
100
00
0.5
90
10
0.5
80
20
0.5
75
25
0.5
5.0
10
5.0
20
5.0
25
5.0
99
Experimental
Table 3.20: Typical formulations of EB curing coating systems with varying ratio
of oligomer (PUA13)
Reactive Diluents (%)
Urethane acrylate
Adhesion
oligomer (%)
Promoter (wt %)
95
TMPTA
EGDMA
HEA
0.5
05
05
05
90
0.5
10
10
10
85
0.5
15
15
15
80
0.5
20
20
20
75
0.5
25
25
25
100
Experimental
EB dose
(KGy)
100 %
10
Tacky
30
Tacky
40
Slightly Tacky
60
Slightly Tacky
70
Non Tacky
80
Table 3.22: EB curing and evaluation of film characteristics at varying dose rate
and reactive diluents (PUA13)
Results after irradiation to EB doses (KGy)
TMPTA
EGDMA
HEA
10 20 30 50 70
30 40 50 70
50 60 70 80
10
10
10
15
15
15
20
20
20
25
25
25
101
Experimental
TMPTA (%)
oligomer (%)
promoter (wt %)
100
00
0.5
95
05
0.5
90
10
0.5
85
15
0.5
80
20
0.5
75
25
0.5
102
Adhesion
Experimental
EB dose
(KGy)
100 %
10
Tacky
30
Tacky
40
Slightly Tacky
60
Slightly Tacky
70
Non Tacky
80
Table 3.25: EB curing and evaluation of film characteristics at varying dose rate
and reactive diluents (GUA4)
TMPTA
(%)
40
50
60
70
05
10
15
20
25
103
Experimental
Table 3.26: Typical formulations of EB curing coating systems with varying ratio
of oligomer (BUA2)
Urethane acrylate
TMPTA (%)
oligomer (%)
promoter (wt %)
100
00
0.5
90
10
0.5
80
20
0.5
75
25
0.5
104
Adhesion
Experimental
Table 3.27: EB curing and evaluation of film characteristics at varying dose rate
(BUA2)
TMPTA
(%)
120
130
140
150
00
10
20
25
105
Experimental
TMPTA (%)
oligomer (%)
Adhesion
promoter (wt %)
100
00
0.5
90
10
0.5
80
20
0.5
75
25
0.5
Table 3.29: EB curing and evaluation of film characteristics at varying dose rate
(NUA2)
TMPTA
(%)
80
90
110
120
00
10
20
25
106
Experimental
107
Experimental
TMPTA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
30 kGy
EGDMA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
108
50 kGy
Experimental
HEA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
70 kGy
TMPTA
TPGDA
NanoAl
NanoAl
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
109
30 kGy
Experimental
EGDMA
TPGDA
NanoAl
NanoAl
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
50 kGy
HEA
TPGDA
NanoAl
NanoAl
EB
(%)
(RD)
content (%)
dispersion (%)
content (%)
Cured
15.00
00
14.50
0.5
1.0
0.5
14.00
1.0
2.0
1.0
13.50
1.5
3.0
1.5
13.00
2.0
4.0
2.0
12.50
2.5
5.0
2.5
85
110
70 kGy
Experimental
TMPTA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
(%)
dispersion (%)
content (%)
Cured
20.00
00
19.50
0.5
1.0
0.5
19.00
1.0
2.0
1.0
18.50
1.5
3.0
1.5
80
60
kGy
18.00
2.0
4.0
2.0
17.50
2.5
5.0
2.5
17.00
3.0
6.0
3.0
16.50
3.5
7.0
3.5
111
Experimental
TMPTA
TPGDA
NanoAl
NanoAl
EB
(%)
(RD)
(%)
dispersion (%)
content (%)
Cured
20.00
00
19.50
0.5
1.0
0.5
19.00
1.0
2.0
1.0
18.50
1.5
3.0
1.5
80
60
KGy
18.00
2.0
4.0
2.0
17.50
2.5
5.0
2.5
17.00
3.0
6.0
3.0
112
Experimental
TMPTA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
(%)
dispersion (%)
content (%)
Cured
20.00
00
19.0
1.0
2.0
1.0
18.0
2.0
4.0
2.0
17.0
3.0
6.0
3.0
16.0
4.0
8.0
4.0
15.0
5.0
10.0
5.0
14.0
6.0
12.0
6.0
13.0
7.0
14.0
7.0
80
140kGy
TMPTA
TPGDA
NanoAl
(%)
(RD)
(%)
dispersion (%)
20.0
00
19.0
1.0
2.0
1.0
18.0
2.0
4.0
2.0
17.0
3.0
6.0
3.0
16.0
4.0
8.0
4.0
15.0
5.0
10.0
5.0
80
EB
140
KGy
113
NanoAl
Experimental
TMPTA
TMPTA
NanoSi
NanoSi
EB
(%)
(RD)
(%)
dispersion (%)
content (%)
Cured
20.0
00
19.0
1.0
2.0
1.0
18.0
2.0
4.0
2.0
17.0
3.0
6.0
3.0
80
110
KGy
16.0
4.0
15.0
5.0
14.0
6.0
8.0
10.0
12.0
114
4.0
5.0
6.0
Experimental
TMPTA
TPGDA
NanoAl
NanoAl
EB
(%)
(RD)
(%)
dispersion (%)
content (%)
Cured
20.0
00
19.0
1.0
2.0
1.0
18.0
2.0
4.0
2.0
110
KGy
80
17.0
3.0
6.0
3.0
16.0
4.0
8.0
4.0
15.0
5.0
10.0
5.0
Experimental
116
Experimental
Experimental
Experimental
according to the ASTM standards. The amount of coated area retained under the tape
corresponds to the adhesion efficiency of the coating. The more coated material removed by
the tape, the poorer the adhesion of the coating to the substrate.
3.8.2.7 Tensile strength properties of thin films (ASTM D882)
In this test method the material is pulled until it breaks in order to measure elongation, tensile
modulus, tensile yield strength and elongation at break (Universal Testing Instrument,
LLOYD INSTRUMENTS, LR 50K, UK). However, it is designed specifically for thin film
less than 1mm (0.04 inch) thick. In this the specimens are rectangular strips of film and are
not dumbbell or dogbone shaped. The average of at least five measurements for each
sample was reported, the experimental error is +/- 10%.
Experimental
sunlight because they produce energy in the UV, visible and infrared regions
(Solarbox 1500e). The results are reported in terms of % gloss retention. The results
were noted in terms of % gloss retention after every 100 hrs upto 500 hrs.
3.8.3.2 QUV accelerated weathering testing (ASTM D4329)
Accelerated weathering simulates damaging effects of long term outdoor exposure of
materials and coatings by exposing test samples to varying conditions of the most
aggressive components of weathering- ultraviolet radiation, moisture and heat. A
QUV test chamber uses fluorescent lamps to provide a radiation spectrum centered in
the ultraviolet wavelengths. Moisture is provided by forced condensations and
temperature is controlled by heaters (Q-Panel Lab products, Europe). The results were
noted in terms of % gloss retention after every 100 hrs up to 500 hrs.
3.8.3.3 Salt spray testing (ASTM B117)
Corrosion resistance effect on long term exposure especially in a automotive
applications is studied in ASTM B117. In this 5% NaCl solution is prepared and
sprayed in the corrosion Box from UK.
3.8.3.4 Chemical resistance
Resistance to acid and alkali was determined by using ASTM D-4274-88 standard
while for detergent resistance standard ASTM D-2248a was followed. For this test,
the coated panels were immersed in 5% solution of HCL (acid), 5% solution of NaOH
(alkali) and 5% solution of detergent. The immersed panels were maintained at
constant temperature. The panels were removed for examination after 6, 12, 18 and 24
hours from the start of the test and observed loss of adhesion, blistering, popping or
any other deterioration of the film.
3.8.3.5 Solvent resistance
The resistance of the coating towards the solvents like methyl ethyl ketone (MEK)
and xylene was determined as per the procedure given in ASTM D-5402-93. The
coated panels were rubbed with the cotton moist with the respective solvent and
observed for any softness of the film, peeling of the film and loss of gloss etc
120
Experimental
121